本文用微扩散法分离并测定微量样品中的氟。以高氯酸为扩散剂使氟成为氟化氢扩散逸出而分离。讨论了扩散条件、器皿及干扰元素的影响,制定了取样量为0.2～2毫克时分离测定0.x～10%氟的方法。此法优点是:仪器简单、快速、准确度好,用简捷的方法对微量磷灰石中氟进行测定,可得满意的结果。 In this paper, micro-diffusion method was used to separate and determine fluorine in trace samples. Perchloric acid as a diffusion agent to make hydrogen fluoride diffusion escape and separation. The effects of diffusion conditions, vessels and interfering elements were discussed. A method for the separation and determination of 0.x ~ 10% fluorine with a sampling volume of 0.2-2 mg was developed. Advantages of this method are: the instrument is simple, fast, accurate, with a simple method of determination of trace amounts of apatite fluoride, satisfactory results can be obtained.